JPH10132763A - Method for automatically adjusting position of sample in x-ray diffraction apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To automatically adjust the position of a sample in an X-ray diffraction apparatus. SOLUTION: A sample 4 is cooled to be subjected to an X-ray diffraction measurement in a low temperature area in the X-ray diffraction apparatus. According to the method, the position of the sample 4 is automatically adjusted at this time. While predetermined three coordinate axes orthogonal to one another are set as X-axis, Y-axis and Z-axis, when the sample is moved in a predetermined range in a YZ direction with X rays being projected to the sample in parallel to the X-axis, a position where an intensity of diffraction rays is maximum is detected. The sample 4 is moved to the position (YZ position adjustment process). Then, the sample 4 is moved in an XZ direction within a predetermined range while the X rays are projected to the sample 4 in parallel to the Y-axis, and a position where the intensity of diffraction rays is maximum is detected. The sample 4 is moved to the position (XZ position adjustment process). The sample 4 is gradually cooled. The YZ position adjustment process and XZ position adjustment process are repeated until the sample 4 reaches a predetermined temperature, thereby, the position of the sample 4 is automatically adjusted.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an automatic sample position adjusting method for automatically adjusting the position of a sample in an X-ray diffraction apparatus for performing X-ray diffraction measurement in a low temperature range by cooling the sample.
For example, it can be applied to a cryogenic X-ray diffractometer using a cryostat.

[0002]

2. Description of the Related Art Single crystal X in a cryogenic temperature region (10K or less)
X-ray diffraction experiments were carried out using a cryostat.
t) is used. The low-temperature source used in the cryostat includes a cryogen storage method, a cryogen continuous flow method, a refrigerator method, and the like, and the sample cooling method includes a conduction cooling method, a gas atmosphere method, and the like.

FIG. 4 shows an example of a conventional cryostat and an X-ray diffraction apparatus.
Comprises a cooling unit 2, a sample holder 3, an airtight case 5, an X-ray transmission window 6, a heater 7, a temperature sensor 8, and the like. The X-ray diffraction apparatus includes a goniometer base 10, a sample rotating base 11, and an X-ray It comprises a generator 12, an X-ray counter 13, and the like.

In the cryostat 1 shown in FIG. 4, a sample holder 3 is fixed to the tip of a cooling unit 2 forming a head of a cooler for obtaining a low temperature by repeating adiabatic compression and expansion while circulating helium gas in a closed circuit. The sample 4 is placed in the sample holder 3.
Is to be attached.

The cooling unit 2 is covered with a cylindrical airtight case 5 for keeping the inside of the airtight vacuum, and near the lower part of the airtight case 5, a X-ray for irradiating the sample 4 is transmitted. An X-ray transmission window 6 is provided. In addition, airtight case 5
The lower end of the sample 4 is fixed to the sample turntable 8, and the sample 4 is placed on both sides of the goniometer base 10 with the sample turntable 11 interposed therebetween.
An X-ray generator 12 that irradiates X-rays through the X-ray transmission window 6 and an X-ray counter 13 that detects diffracted X-rays from the sample 4 through the X-ray transmission window 6 are provided. The X-ray counter 13 is rotatable around the sample 4 at a predetermined angular velocity, and the X-ray transmission window 6 is formed at a central angle of about 190 ° in the circumferential direction of the airtight case 5.

A cooling part 2a formed at the lower end of the cooling part 2
A temperature sensor 8 is mounted on the upper surface of the sample 4, and the temperature sensor 8 detects the temperature of the sample 4 at the time of the X-ray diffraction measurement to control the temperature of the cooling portion 2a. Also,
A heater 7 is wound just above the cooling portion 2a, and the temperature of the sample 4 can be controlled by the heater 7.

When the measurement is performed with such a cryostat 1 and an X-ray diffractometer, the sample 4 is mounted on the sample holder 3 in a state where the airtight case 5 is removed at room temperature, and then the airtight case is mounted, and then the cooling is performed. Had to do it.

[0008]

The material of the X-ray transmission window 6 is Be or fiber reinforced plastic (fiber rei).
nforced plastics) is used. For this reason, the position of the sample 4 inside cannot be confirmed from the outside.

On the other hand, when the cryostat 1 is set at a low temperature, the position of the sample 4 moves due to the contraction and deformation of the cooling unit 2. When the sample 4 is cooled from room temperature to extremely low temperature, the position of the sample may move in the order of mm.

Conventionally, such adjustment of the position of the sample 4 is performed manually, which is very troublesome. In addition, even if an attempt is made to adjust the sample position by a motor or the like, an adjusting person skilled in adjustment work has to perform adjustment each time measurement is performed.

The present invention has been made to solve the above problems, and has as its object to provide an automatic sample position adjusting apparatus for automatically adjusting the position of a sample in an X-ray diffraction apparatus.

[0012]

According to the first aspect of the present invention, there is provided a method for automatically adjusting the position of a sample in an X-ray diffraction apparatus for performing X-ray diffraction measurement in a low temperature range by cooling the sample. When three predetermined coordinate axes orthogonal to each other are set to an X axis, a Y axis, and a Z axis, respectively,
A YZ position adjusting step of moving the sample in a predetermined range in the YZ direction while irradiating X-rays in parallel with the axis to find a position where the intensity of the diffraction line is maximized, and moving the sample to that position; XZ position adjustment that moves the sample within a predetermined range in the XZ direction while irradiating X-rays in parallel with the Y axis to find the position where the intensity of the diffraction line is maximum, and moves the sample to that position. And adjusting the position of the sample automatically by repeating the YZ position adjustment step and the XZ position adjustment step until the sample reaches a predetermined temperature while gradually cooling the sample. .

[0013]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, an embodiment of a method for automatically adjusting a sample position in an X-ray diffraction apparatus according to the present invention will be described in detail with reference to the drawings.

FIG. 1 shows the configuration of an X-ray diffraction apparatus and a cryostat according to the present embodiment. The components other than the X-axis adjustment device 20, the Y-axis adjustment device 21, and the Z-axis adjustment device 22 function in the same manner as in the related art, and a description thereof will be omitted.

The X-axis adjusting device 20 includes a cryostat 1
Is a device for finely adjusting the position of the sample in the X-axis direction, and is attached between the cryostat 1 and the sample turntable 11,
It is controlled by the control device as described later.
Similarly, the Y-axis adjustment device 21 and the Z-axis adjustment device 22 are devices for finely adjusting the position of the cryostat 1 in the Y-axis and Z-axis directions, respectively.
And is controlled by a controller.

Here, the Z axis is a coordinate axis perpendicular to the rotation plane of the sample turntable 11. The X axis is a coordinate axis perpendicular to the Z axis, and the Y axis is a coordinate axis perpendicular to both the X axis and the Z axis.

FIG. 2 shows a schematic configuration of the control device. The control device 30 includes a central processing unit 31, a main storage device 32, an auxiliary storage device 33, a keyboard interface 34, a mouse interface 35, and a display interface. 36 and input / output interface 37
The control device 30 includes a keyboard 40, a mouse 41, and a display device 42.
Connected through. The same and corresponding parts as those in FIG. 1 are denoted by the same reference numerals. In the present embodiment, each unit of the cryostat 1 and the X-ray diffraction device is controlled by the control device 30 and software running on the central processing unit 31.

The input / output interface 37 is an interface for connecting the control device 30, the cryostat 1, and each part of the X-ray diffraction device. In FIG. 2, the X-axis adjustment device 20, the Y-axis adjustment device 21, and the Z-axis adjustment device Device 22
And the X-ray counter 13 are connected. Actually, the cryostat 1 and other parts of the X-ray diffraction apparatus are also connected to the input / output interface 37, but the description of those parts will be omitted.

The operation for adjusting the position of the sample with such a configuration will be described below with reference to the flowchart of FIG.

First, the sample 4 is mounted on the sample holder 3, and the sample is gradually cooled from room temperature.

The control device 30 controls each part of the X-ray diffractometer, the X-ray generator 12 irradiates the sample 4 with X-rays in parallel with the X-axis, and the X-ray counter 13 converts the diffracted rays. (Step 301).

The control device 30 controls the Y-axis adjustment device 21 and the Z-axis adjustment device 22 via the input / output interface 37 to move the cryostat 1 in parallel with the YZ plane, and scan a predetermined range on the YZ plane. I do. During the scan, the X-ray counter 13 sends the intensity of the diffraction line to the controller 30 via the input / output interface 37, and the controller 3
0 stores the strength and the amount of movement of the cryostat 1 in the Y-axis and Z-axis directions at that time in the main storage device 32 or the auxiliary storage device 33 (step 302).

After the scanning of the predetermined range on the YZ plane is completed, the control device 30 detects a peak from the stored intensities of the diffraction lines (searches for the highest intensity) and sets the Y-axis and the Y-axis at that time. The amount of movement of the cryostat 1 in the Z-axis direction is obtained, and the Y-axis adjustment device 21 and the Z-axis adjustment device 22 are controlled to move the cryostat 1 to a position where the intensity of the diffraction line becomes maximum. After the movement is completed, the control device 30 deletes the data of the strength and the movement amount of the cryostat 1 in the Y-axis and Z-axis directions (Step 303).

The control device 30 controls each part of the X-ray diffraction device, the X-ray generation device 12 irradiates the sample 4 with X-rays in parallel with the Y-axis, and the X-ray counting device 13 converts the diffraction lines. (Step 304).

The control device 30 controls the X-axis adjustment device 20 and the Z-axis adjustment device 22 via the input / output interface 37 to move the cryostat 1 in parallel with the XZ plane and scan a predetermined range on the XZ plane. I do. During the scan, the X-ray counter 13 sends the intensity of the diffraction line to the controller 30 via the input / output interface 37, and the controller 3
0 stores the strength and the amount of movement of the cryostat 1 in the X-axis and Z-axis directions at that time in the main storage device 32 or the auxiliary storage device 33 (step 305).

After the scanning of the predetermined range on the XZ plane is completed, the control device 30 detects a peak from the stored diffraction line intensities (searches for the highest intensity), and determines the X-axis at that time. The amount of movement of the cryostat 1 in the Z-axis direction is obtained, and the X-axis adjustment device 20 and the Z-axis adjustment device 22 are controlled to move the cryostat 1 to a position where the intensity of the diffraction line becomes maximum. After the movement is completed, the control device 30 deletes the data of the strength and the movement amount of the cryostat 1 in the X-axis and Z-axis directions (Step 306).

When the cooling of the sample 4 has reached a steady state, the adjustment of the sample position is terminated. If not, the process returns to step 301 to perform the adjustment again (step 307).

As described above, according to the above embodiment,
A process of moving the sample to a position where the intensity of the diffraction line in the YZ direction is maximized while gradually cooling the sample from room temperature;
The process of moving the sample to the position where the intensity of the diffraction line in the Z direction is maximized is repeated until the temperature of the sample reaches a steady state, so that the position of the sample 4 can be automatically adjusted very easily. Will be possible.

The present invention is not limited to the above embodiment, but allows various modifications.

The present invention can be applied not only to the cryostat shown in the above embodiment, but also to other cryostats. The low-temperature source used for the applicable cryostat includes a cryogen storage method, a cryogen continuous flow method, a refrigerator method, and the like, and a sample cooling method includes a conduction cooling method, a gas atmosphere method, and the like.

Further, the X-ray counter according to the present invention has a CC
The present invention can be applied to any device capable of counting X-rays, such as a D (charge coupled device) camera, an X-ray film, a flat plate or a cylindrical IP (Imaging Plate), and a reader thereof.

Further, in the above embodiment, the X-axis adjustment device, the Y-axis adjustment device, and the Z-axis adjustment device are provided between the cryostat and the sample rotating table, but they may be provided at other places. Further, the relative positional relationship between the X-axis adjustment device, the Y-axis adjustment device, and the Z-axis adjustment device may be arbitrarily determined.

[0033]

As described above, according to the present invention, the predetermined three coordinate axes orthogonal to each other are set to the X axis and the Y axis, respectively.
When the sample is gradually cooled, the sample is irradiated with X-rays in parallel with the X axis, and the sample is placed in the YZ direction.
Moving the sample within a predetermined range in the direction to find the position where the intensity of the diffraction line is maximum, and moving the sample to that position; and irradiating the sample with X-rays in parallel with the Y axis. The process of moving the sample in the XZ direction within a predetermined range to find a position where the intensity of the diffraction line is maximum, and moving the sample to that position is repeated until the sample reaches a predetermined temperature, and the position of the sample is automatically set. , The position of the sample of the X-ray diffractometer can be automatically adjusted very easily.

[Brief description of the drawings]

FIG. 1 is a front sectional view of an X-ray diffraction apparatus and a cryostat according to an embodiment.

FIG. 2 is a block diagram illustrating a schematic configuration of a control device according to the embodiment.

FIG. 3 is a flowchart showing an operation when performing automatic sample position adjustment of a sample in the embodiment.

FIG. 4 is a front sectional view of a conventional X-ray diffraction apparatus and a cryostat.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Cryostat 10 Goniometer base 11 Sample turntable 12 X-ray generator 13 X-ray counter 20 X-axis adjuster 21 Y-axis adjuster 22 Z-axis adjuster 30 Controller

Claims (1)

[Claims] 1. An automatic sample position adjusting method for automatically adjusting the position of a sample in an X-ray diffractometer for performing X-ray diffraction measurement in a low temperature range by cooling the sample, comprising: three predetermined coordinate axes orthogonal to each other To the X axis and Y
When the sample is irradiated with X-rays in parallel with the X axis,
A YZ position adjustment step of moving the sample in the predetermined direction in the Z direction to find a position where the intensity of the diffraction line is maximized and moving the sample to that position, and irradiating the sample with X-rays in parallel with the Y axis. X
An XZ position adjustment step of moving the sample in the predetermined direction in the Z direction to find the position where the intensity of the diffraction line is maximum, and moving the sample to that position. A method for automatically adjusting the position of a sample in an X-ray diffraction apparatus, wherein the position of the sample is automatically adjusted by repeating the position adjusting step and the XZ position adjusting step until the sample reaches a predetermined temperature.